JP2012531304A - 高温で化学反応を連続的に行うための装置 - Google Patents
高温で化学反応を連続的に行うための装置 Download PDFInfo
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Abstract
Description
マイクロ波による反応混合物の照射は、加熱管として、円筒形空洞共振器(60×10cm)内に軸対称に位置するセラミック管(60×1cm)を含む装置内で実施した。空洞共振器の1端面で、この加熱管が、結合アンテナとして機能する内部導体管の空洞を通って延びている。マグネトロンによって生じる、周波数2.45GHzのマイクロ波場が、結合アンテナにより空洞共振器内に結合され(E01空洞照射器、単一モード)、その中で定常波が形成された。加熱された反応混合物は続いてすぐに、断熱された特殊鋼管(特記しない限り、3.0m×1cm)を通って運ばれた。反応管を出た後、反応混合物は大気圧まで減圧され、直ちに集中熱交換器により約60℃まで冷却された。
撹拌器、内部温度計および圧力調整器を備える10lのビュッヒ撹拌オートクレーブ中にラウリル酸3.4kg(17mol)を投入し、60℃に加熱し、わずかに冷却しながらN,N−ジメチルアミノプロピルアミン2.6kg(25.5mol)を慎重に混ぜた。
ガス注入管、撹拌器、内部温度計および圧力調整器を備える10lのビュッヒ撹拌オートクレーブ中にココ油4.2kg(5.5mol、分子量764g/mol)を投入し、45℃に加熱した。この温度にて、ジエチルアミン2.0kg(27mol)および触媒としてナトリウムエチラート100gをゆっくり添加し、撹拌しながら均質化した。
撹拌器、内部温度計および圧力調整器を備える10lのビュッヒ撹拌オートクレーブ中にキャノーラ油脂肪酸3.1kg(10mol、分子量309g/mol)を投入し、メタノール2.58kg(80mol)およびメタンスルホン酸0.075kgを混合した。こうして得られた反応混合物を35バールの動作圧力にて10.01l/hで連続的に前記装置中をポンプ圧送し、加熱ゾーンにおいて2.6kWのマイクロ波電力にさらすと、その92%が反応物によって吸収された。反応混合物の加熱ゾーンにおける滞留時間は約17秒であり、反応区域における滞留時間は約86秒であった。加熱ゾーンの端部で反応混合物は251℃の温度を有し、反応区域を出た後では245℃の温度を有した。
窒素不活性化処理(Stickstoffinertisierung)した1lの三つ口フラスコにエタノール500mlを投入し、強く撹拌しながらその中にテトラキス(トリフェニルホスフィン)パラジウム(0)50g(44mmol)を微細に懸濁させた。撹拌器、内部温度計および圧力調整器を有する、窒素で不活性化処理した10lのビュッヒ撹拌オートクレーブ中に、エタノール/水/ジメチルホルムアミドの混合物2リットルを投入し、その中に4−ブロモトルエン376g(2.2mol)およびフェニルボロン酸244g(2.0mol)を溶解した。続いて窒素不活性化処理の下で、この触媒懸濁液を撹拌オートクレーブにゆっくりと加え、均質に撹拌した。こうして得られた容易にポンプ給送可能な懸濁液を30バールの動作圧力にて1.5l/hで連続的に前記装置中をポンプ圧送し、加熱ゾーンにおいて1.2kWのマイクロ波電力にさらすと、その92%が反応物によって吸収された。反応混合物の加熱ゾーンにおける滞留時間は約113秒であり、反応区域における滞留時間は約10分であった。加熱ゾーンの端部で反応混合物は255℃の温度を有し、反応区域を出た後では251℃の温度を有した。
撹拌器、内部温度計および圧力調整器を有する10lのビュッヒ撹拌オートクレーブ中に、ポリ(イソブチレン)4.0kg(Glissopal(登録商標)1000、BASF AG、分子量1000、α位二重結合含有量80%、4.0mol)を投入し、無水マレイン酸431g(4.4mol)を混合し、撹拌しながら約70℃に加熱した。
これらの実験においては、上記の加熱ゾーンのみを用いて、すなわち、反応管を使用せずに実験1〜5を繰り返した。対応する実験パラメータを表1にまとめた。列挙した温度は、加熱ゾーンを出る際に測定された値である。
Claims (19)
- マイクロ波発生器、内部にマイクロ波透過性管があるマイクロ波アプリケータ、及び等温反応区域を含む、化学反応を連続的に行うための装置であって、前記マイクロ波透過性管内の反応物が、加熱ゾーンとして機能するマイクロ波アプリケータ中を通って誘導され、前記マイクロ波アプリケータ中では、マイクロ波発生器から前記マイクロ波アプリケータへ誘導されるマイクロ波を使って、該反応物が反応温度まで加熱され、そして加熱され、そして場合によっては圧力下にある該反応物が、前記加熱ゾーンから出た直後に前記加熱ゾーンに直接つながる等温反応区域中に移され、そしてその等温反応区域から出た後に冷却されるように、前記マイクロ波発生器、前記マイクロ波アプリケータ、及び前記等温反応区域が配置されている、上記の装置。
- 前記マイクロ波透過性反応管が、単一モード(Monomode)のマイクロ波アプリケータの内部に存在する、請求項1に記載の装置。
- 前記マイクロ波透過性管の長軸が、単一モードのマイクロ波アプリケータのマイクロ波伝播方向にある、請求項1及び/又は2に記載の装置。
- 前記マイクロ波透過性反応管が、導波体を介してマイクロ波発生器と接続された中空導波管の内部に存在する、請求項1〜3のいずれか一つに記載の装置。
- 前記マイクロ波アプリケータが空洞共振器として形成されている、請求項1〜4のいずれか一つに記載の装置。
- 前記マイクロ波アプリケータが反射型の空洞共振器として形成されている、請求項1〜5のいずれか一つに記載の装置。
- 前記反応管が、中空導波管の中心対称軸と軸を合わせて配列される、請求項1〜6のいずれか一つに記載の装置。
- 前記空洞共振器が、マイクロ波の同軸遷移部を有する、請求項1〜7のいずれか一つに記載の装置。
- 前記空洞共振器がE01nモードで稼働され、その際、nは1〜200の整数である、請求項1〜8のいずれか一つに記載の装置。
- 十分にマイクロ波透過性の反応管が、マルチモードマイクロ波アプリケータの内部にある、請求項1に記載の装置。
- 前記等温反応区域が断熱管である、請求項1〜10のいずれか一つに記載の装置。
- 前記等温反応区域が、エネルギーを供給又は放出するための装置を含む、請求項1〜11のいずれか一つに記載の装置。
- 化学反応を連続的に行うための方法であって、請求項1〜12のいずれか一つに記載の装置内の反応物が、加熱ゾーンを介して誘導され、該加熱ゾーンでは、その反応物がマイクロ波を使って反応温度まで加熱され、そして加熱されかつ場合によっては圧力下にある前記反応物が、前記加熱ゾーンから出た直後にその加熱ゾーンに隣接する等温反応区域に移送され、そしてその等温反応区域から出た後に冷却される、上記の方法。
- 前記化学反応が、−20kJ/mol未満の反応熱によって特徴づけられる、請求項13に記載の方法。
- 前記化学反応が、吸熱性である、請求項13及び14のいずれか一つに記載の方法。
- 前記反応物が、マイクロ波照射によって70〜500℃の温度に加熱される、請求項13〜15のいずれか一つに記載の方法。
- 前記マイクロ波照射が、大気圧超の圧力で遂行される、請求項13〜16のいずれか一つに記載の方法。
- 前記等温反応区域が、反応区域を通過した後の反応物の温度が、その進入温度に比べて最大で±30℃だけ異なるという性質をしている、請求項13〜17のいずれか一つに記載の方法。
- 前記空洞共振器中で定常波が形成される、請求項13〜18のいずれか一つに記載の方法。
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JP2012531449A (ja) * | 2009-06-30 | 2012-12-10 | クラリアント・ファイナンス・(ビーブイアイ)・リミテッド | 芳香族カルボン酸のアミドの連続的製法 |
JP2013505275A (ja) * | 2009-09-22 | 2013-02-14 | クラリアント・ファイナンス・(ビーブイアイ)・リミテッド | 連続的エステル交換方法 |
JP2014182930A (ja) * | 2013-03-19 | 2014-09-29 | Saida Fds Inc | 流通管及びこの流通管を備えたマイクロ波装置 |
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DE102006047619B4 (de) * | 2006-10-09 | 2008-11-13 | Clariant International Limited | Verfahren zur Herstellung basischer Fettsäureamide |
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DE102008017216B4 (de) * | 2008-04-04 | 2013-08-14 | Clariant International Ltd. | Kontinuierliches Verfahren zur Herstellung von Fettsäureamiden |
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DE102008017214B4 (de) * | 2008-04-04 | 2012-02-16 | Clariant International Limited | Kontinuierliches Verfahren zur Herstellung von Fettsäurealkanolamiden |
DE102008017217A1 (de) * | 2008-04-04 | 2009-10-08 | Clariant International Ltd. | Kontinuierliches Verfahren zur Herstellung von Amiden aromatischer Carbonsäuren |
DE102009042523B4 (de) | 2009-09-22 | 2012-02-16 | Clariant International Ltd. | Vorrichtung und Verfahren zur kontinuierlichen Durchführung heterogen katalysierter chemischer Reaktionen bei hohen Temperaturen |
DE102010056565A1 (de) | 2010-12-30 | 2012-07-05 | Clariant International Ltd. | Verfahren zur Modifizierung Hydroxylgruppen tragender Polymere |
DE102010056564A1 (de) | 2010-12-30 | 2012-07-05 | Clariant International Limited | Hydroxylgruppen und Estergruppen tragende Polymere und Verfahren zu ihrer Herstellung |
DE102011102975A1 (de) * | 2011-05-31 | 2012-12-06 | Linde Aktiengesellschaft | Reaktoreinrichtung |
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DE102009031053A1 (de) | 2009-06-30 | 2011-01-13 | Clariant International Ltd. | Kontinuierliches Verfahren zur Herstellung von Estern aliphatischer Carbonsäuren |
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DE102010056579A1 (de) | 2010-12-30 | 2012-07-05 | Clariant International Limited | Kontinuierliches Verfahren zur Umsetzung Säuregruppen tragender Polymere mit Aminen |
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DE102010056566A1 (de) | 2010-12-30 | 2012-07-05 | Clariant International Ltd. | Kontinuierliches Verfahren zur Veresterung Säuregruppen tragender Polymere |
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2009
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JP2012531449A (ja) * | 2009-06-30 | 2012-12-10 | クラリアント・ファイナンス・(ビーブイアイ)・リミテッド | 芳香族カルボン酸のアミドの連続的製法 |
JP2013505275A (ja) * | 2009-09-22 | 2013-02-14 | クラリアント・ファイナンス・(ビーブイアイ)・リミテッド | 連続的エステル交換方法 |
JP2014182930A (ja) * | 2013-03-19 | 2014-09-29 | Saida Fds Inc | 流通管及びこの流通管を備えたマイクロ波装置 |
Also Published As
Publication number | Publication date |
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AU2010268445A1 (en) | 2011-11-03 |
WO2011000460A2 (de) | 2011-01-06 |
PL2448663T3 (pl) | 2013-09-30 |
EA201200070A1 (ru) | 2012-05-30 |
EP2448663A2 (de) | 2012-05-09 |
CA2766950A1 (en) | 2011-01-06 |
MX2011011736A (es) | 2011-11-29 |
BRPI1014323A2 (pt) | 2016-04-05 |
EP2448663B1 (de) | 2013-04-17 |
CN102448603A (zh) | 2012-05-09 |
KR20120090024A (ko) | 2012-08-16 |
ES2406760T3 (es) | 2013-06-10 |
AU2016204757A1 (en) | 2016-07-28 |
US8974743B2 (en) | 2015-03-10 |
DE102009031059A1 (de) | 2011-01-05 |
US20120088885A1 (en) | 2012-04-12 |
WO2011000460A3 (de) | 2011-03-31 |
JP2016021399A (ja) | 2016-02-04 |
EA021427B1 (ru) | 2015-06-30 |
CN102448603B (zh) | 2015-05-13 |
JP5996736B2 (ja) | 2016-09-21 |
MY152996A (en) | 2014-12-31 |
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